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Ammonium Hydroxide → racemic 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzamide

HRID 595319
Notes
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Reaction equation

HRID 595319 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([C:15]2[CH:16]=[N:17][N:18]([CH:20]([C:22]3[CH:30]=[CH:29][C:25]([C:26](O)=[O:27])=[CH:24][CH:23]=3)[CH3:21])[CH:19]=2)[CH:5]=[C:6]([NH:8][C:9]2[N:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:7]=1.[OH-].[NH4+:32]>C1COCC1.CN(C=O)C.C(OCC)(=O)C.O>[CH3:1][C:2]1[CH:3]=[C:4]([C:15]2[CH:16]=[N:17][N:18]([CH:20]([C:22]3[CH:30]=[CH:29][C:25]([C:26]([NH2:32])=[O:27])=[CH:24][CH:23]=3)[CH3:21])[CH:19]=2)[CH:5]=[C:6]([NH:8][C:9]2[N:10]=[CH:11][CH:12]=[CH:13][N:14]=2)[CH:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 2

HCID 14923Ammonium HydroxideHCID 1182088364-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzoic acid

Product 1

HCID 118208806racemic 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzamide

Reagents, catalysts & solvents 4

HCID 962WaterSolventHCID 6228Dimethylformamide
Solvent
HCID 8028TetrahydrofuranSolvent
HCID 8857Ethyl AcetateSolvent

Procedure

2-(1H-Benzo[d][1,2,3]triazol-1-yl)-1,1,3,3-tetramethylisouronium tetrafluoroborate (101 mg, 0.315 mmol) was added to a solution of 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzoic acid (105 mg, 0.263 mmol) in THF (5.0 mL) and DMF (1.0 mL). Ammonium hydroxide (0.15 mL, 1.05 mmol) was then added and the reaction mixture was stirred at ambient temperature for 1 hour. The reaction mixture was diluted with ethyl acetate (100 mL) and water (10 mL). The organic layer was separated and washed with water (2×10 mL) followed by brine (10 mL). The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to afford the crude product residue. The crude product residue was purified by column chromatography on silica (0-100% [5% methanol in ethyl acetate]/hexanes) to afford racemic 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzamide. MS ESI calcd. for C23H23N6O [M+H]+ 399. found 399. 1H NMR (500 MHz, DMSO-d6) δ 9.46 (s, 1H), 8.46 (d, J=5.0 Hz, 2H), 8.22 (s, 1H), 7.92 (s, 1H), 7.82 (s, 1H), 7.79 (d, J=6.5 Hz, 2H), 7.71 (s, 1H), 7.41 (s, 1H), 7.36-7.26 (m, 3H), 7.00 (s, 1H), 6.80 (t, J=5.0 Hz, 1H), 5.70-5.64 (m, 1H), 2.27 (s, 3H), 1.83 (d, J=7.0 Hz, 3H).

Workup

  1. customThe organic layer was separated
  2. washwashed with water (2×10 mL)
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto afford the crude product residue
  7. customThe crude product residue was purified by column chromatography on silica (0-100% [5% methanol in ethyl acetate]/hexanes)

Sources & evidence

ORD record
ord-b6f6164b20ba4b069030f6e6f7a54042
Source dataset
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09242984B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes